In situ monitoring of structural changes during the adsorption on flexible porous coordination polymers by X-ray powder diffraction: Instrumentation and experimental results

• In situ instrumentation for combined XRD and adsorption experiments was developed.
• Set-up assure the precise temperature control needed for adsorption experiment.
• CO2 and n-butane adsorption at 273 K up to 1 bar on ELM-11 was investigated.
• For the first time the crystal structures of n-butane@ELM-11 at 273 K is reported.

A new instrumentation for in situ X-ray powder diffraction allows to follow structural changes in the crystal structure of flexible coordination polymers during adsorption and desorption of gases. The system is based on closed cycle He-cryostat that ensures the high temperature stability in the range of 5.5–450 K. The automated gas dosing system facilitates the physisorption measurements in the pressure range of 0.01–130 kPa. The system is implemented on KMC-2 and MAGS beamlines at Helmholtz Zentrum Berlin für Materialien und Energie. Using new instrumentation, the adsorption of CO2 and n-butane at 273 K on a flexible two-dimensional coordination polymer ELM-11 (ELM – Elastic Layer Material) was investigated.

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